稳定同位素标记13C6-结晶紫和13C6-隐色结晶紫的合成

Syntheses of Labeled Crystal Violet and Leucocrystal Violet

摘要:

以13C-甲醇为前体，通过磺酸酯活化方法得到13C2-N,N-二甲基苯胺，再进一步缩合得到13C6-隐色结晶紫和13C6-结晶紫。产品结构经质谱和核磁等表征确定，化学纯度高于99.0 %，同位素丰度高于98.5 %，可作为食品安全领域检测内标试剂。

Abstract:

This article presents efficient syntheses of two labeled standards [13C6]leucocrystal violet and [13C6]violet crystal with 13CH3OH as the common substrate. Esterification of p-toluenesulfonyl chloride with 13CH3OH provided [13C]methyl p-toluenesulfonate, which was used to methylate aniline to give [13C2]N,N-dimethylaniline. Condensation of [13C2]N,N-dimethylaniline afforded [13C6]leucocrystal violet and [13C6]violet crystal. Both products were shown by NMR and LC-MS to be target compounds. Their chemical purities are higher than 99 % and isotopic enrichment are higher than 98.5 %.